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Cng ho x hi ch ngha Vit nam B Nng nGhip v pht trin nng thn _________________________

Tiu chun ngnh 10TCN 452-2001


Phng php xc nh hm lng nitrat v nitrit
Phn tch cy trng

H ni 2001

Nhm C

Tiu chun ngnh

10 TCN 452-

2001

Phn tch cy trng

Phng php xc nh hm lng nitrat v nitrit

1. Phm vi p dng. Tiu chun ny quy nh phng php xc nh hm lng nitrat v nitrit tng s cho cc mu cy trng ti. 2. Nguyn tc. S dng l vi sng ho tan nhanh (chit) nitrat v nitrit (NO3 NO2-) trong mu ti bng nc, un vi sng mc nng lng cao. Xc nh hm lng nitrat bng phng php trc quang, da trn phn ng ca nitrat vi axit disunfophenol to thnh nitrofenoldisunfonic trong mi trng kim c mu vng c trng, o ti bc sng 410nm. Xc nh hm lng nitrit bng phng php trc quang, da trn phn ng ca nitrit vi axit sunfanilic v naphtylamin trong mi trng axit c mu hng, o ti bc sng 540nm. 3. Thit b v thuc th 3.1. Thit b 3.1.1. My quang ph k (Spectrophotometer) 3.1.2. My nghin mu thc vt ti 3.1.3. Cn phn tch chnh xc 0,0002g 3.1.4. L vi sng (Cng xut 850w, tn s hot ng 2450MHz) 3.1.5. Ni cch thu. 3.1.5. Cc loi cc, bnh nh mc 50ml, 100ml, 250ml, 1000ml 3.2. Thuc th 3.2.1. Dung dch axit phenoldisunfonic (*) (*)C th t ch to dung dch axit phenoldisunfonic bng cch: Ho tan 25g phenol tinh khit vo 150ml H2SO4 c (d= 1,84), thm 75ml axit H2SO4 bc khi. un nng 2 gi trong nc si, bo qun trong l mu ti. Cng c th ho tan 30g phenol tinh khit vo 200ml H2SO4 c (d= 1,84), lc u. Sau ni bnh vi ng sinh hn hi lu v un trong 6 gi, bo qun trong l mu ti. 3.2.2. Dung dch thuc th Griss (**)
10TCN 452-2001

(**) Thuc th Griss kiu c-1: Pha dung dch axit Sunfanilic: ho tan 0,5g axit sunfanilic trong 150ml

axit acetic 10%. Pha dung dch naphtylamin: ho tan 0,1g naphtylamin vo 20ml nc ct, khuy u, un si dung dch thu c, lng trong, lc ly phn trong v thm vo phn trong 150ml axit acetic 10% lc u, bo qun trong l mu ti. Hoc kiu c -2: Ho tan 150ml axit acetic 99% vi 350ml nc, tip ho tan thm 0,10g Napthylamin v sau 0,30g axit Sunfanilic, khuy tan v trn u.
(**) Thuc th Griss ci tin: Gm 2 dung dch Sunfanylamit v N(1-naphtyl) etylen diamine dihydrroclorua (NED)
1/ Sunfanylamit: Cn 5g Sunfanylamit ho tan trong bnh nh mc 500ml c cha 50ml HCl c v 300ml nc ct. Pha long n 500ml bng nc ct, lc k. Dung dch n nh trong nhiu thng.

2/ N(1-naphtyl) etylen diamine dihydrroclorua(NED): Cn 0,5g NED ho tan trong 500ml nc ct, bo qun trong bnh ti mu. Dung dch khng bn, thay th hng thng hoc khi chuyn sang mu nu. 3.2.3. Dung dch tiu chun nitrat 10ppm Cn chnh xc 0,1631g KNO3 kh tinh khit, ho tan bng nc v thm nc n 1000 ml trong bnh nh mc. Trn u dung dch, thu c dung dch tiu chun c nng 100mg/lt (100ppm), ho long tip10 ln c dung dch tiu chun nitrat 10ppm. 3.2.4. Dung dch tiu chun nitrit 5ppm Cn chnh xc 0,375g NaNO2 tinh khit v kh, ho tan bng nc thnh 1 lt dung dch, thu c dung dch tiu chun 250ppm NO2-. Pha long 50 ln c dung dch tiu chun 5 ppm NO2-. 3.2.5. Dung dch NH4OH(1:1). Hoc NaOH 10% 3.2.6. Nc khng c NO3- v NO2-, dn in nh hn 2S/cm pH 5,6-7,0 4. Phng php chit nitrat v nitrit bng l vi sng( *** )

Chit NO3- v NO2- bng l vi sng c th loi tr c hu ht cc nh hng xu ti kt qu phn tch nitrat v nitrit. Cch lm nh sau:

Thi nh trn u mu, cn 10g mu cho vo cc 250ml, thm nc ct n khong 200ml.


4.1. Cho cc vo l vi sng v tin hnh un vi sng mc nng lng cao 100% trong thi gian 7 pht (Cng c th un mc nng lng 70% vi thi gian 12 pht). 4.2. Ly ra ngui, lc b b v nh mc dch lc bng nc ct n 200ml. Ly 10ml xc nh NO3 v 10ml xc nh NO2 (***) Tham kho ti liu Nghin cu xc nh hm lng NO3,NO2 ca Phm Huy ng, Trn T Hiu, Ng Huy Du-2000 ) 5. Phng xc nh nitrat: 5.1. Xy dng ng chun NO3 . Dy tiu chun 01ppm NO3
10TCN 452-2001

5.1.1 Chun b mt dy cc 250ml, thm vo mi cc mt lng dung dch nitrat tiu chun nng 10mg/l theo th t ln lt 0,0 ; 0,5 ; 1,0 ; 2,0 ; 3,0 ; 4,0 ; 5,0 ml. 5.1.2 un cch thu cho bay hi n kh cn khng chy, ngui(****)
(****) C th c cn bng l vi sng mc nng lng thp 30%, thi gian mt khong 7-10 pht.

5.1.3 Thm vo mi cc 1ml dung dch axit phenoldisunfonic v lc mnh cho phn ng sy ra nhanh chng. 5.1.4 yn trong 10 pht, sau thm mi cc khong 20ml nc. 5.1.5 Cn thn thm vo mi cc 8ml dung dch NH4OH (1:1) cho pH nm trong khong 1011. (*****)

(*****) C th trung ho dung dch bng cch nh tng git dung dch NaOH 10% (th bng giy qu tm). Dung dch s chuyn mu vng (d mt t NaOH khng nh hng n mu ca dung dch.
5.1.6 Chuyn dung dch trong cc vo bnh nh mc 50ml v nh mc n vch, lc k. 5.1.7 o hp th quang ca dung dch bc sng 410nm. Sau biu din ln th ta c ng chun c NO3 c nng t 0-1ppm NO3 5.2. o mu: 5.2.1 Chun b cc 250ml, ly vo mi cc 10ml dung dch mu chit bng l vi sng(4.3.)

5.2.2 Tip tc cc bc 5.1.2 ... 5.1.6 nh vi dy tiu chun 5.2.3 o hp th quang ca dung dch mu bc sng 410nm. 5.2.4 ng thi tin hnh mu trng vi 10ml nc, nh vi dung dch mu. 5.2.5 o dung dich mu ng nht iu kin vi o dung dch tiu chun. 5.2.6 Cn c vo th tiu chun v s o mu trn my xc nh nng ppmNO3 trong dung dch o, t suy ra hm lng NO3 trong mu 5.3. Cng thc tnh ton: mg NO3-/ kg mu ti = a . V . 1000 v . m

Trong : a: hm lng NO3- trong th tch trch (mg) V: th tch dung dch mu sau khi chit (ml) v: th tch dung dch trch ra xc nh (ml) m: khi lng mu ti (g)
10TCN 452-2001

6. Phng xc nh nitrit: 6.1. Xy dng ng chun NO2 . Dy tiu chun 0 0,5ppm NO2- s dng thuc th Griss kiu c. 6.1.1 Chun b mt dy bnh nh mc 50ml, ln lt thm vo mi bnh mt lng dung dch nitrit tiu chun nng 5ppm theo th t ...0,0 ; 0,5 ; 1,0 ; 2,0 ; 3,0 ; 4,0 ; 5,0 ml. 6.1.2 Thm vo mi bnh 1ml thuc th Sunfanilic v 1ml thuc th naphtylamin. 6.1.3 Ln nh mc bng nc n vch v lc k. 6.1.4 Sau 20 pht o hp th quang ca dung dch bc sng 520nm. Sau biu din ln th ta c ng chun c nng NO2 trong dung dch t 0 - 0,5ppm NO2 (C th dng thuc th Griss ci tin: Mc 6.1.2 thay bng thm vo mi bnh 1ml thuc th Sunfanylamit v 1ml thuc th N(1naphtyl) etylen diamine dihydrroclorua (NED) 6.2 o mu:

6.2.1 Chun b mt dy bnh nh mc 50ml, ln lt thm vo mi bnh 10ml dung dch mu 6.2.2 Thm vo mi bnh 1ml thuc th Sunfanilic v 1ml thuc th naphtylamin. 6.2.3 Ln nh mc bng nc ct n vch v lc k. 6.2.4 Sau 20 pht o hp th quang ca dung dch bc sng 520nm. 6.2.5 ng thi tin hnh mu trng vi 10ml nc, tin hnh nh vi dung dch mu. 6.2.6 o dung dich mu ng nht iu kin vi o dung dch tiu chun. 6.2.7 Cn c vo th tiu chun v s o mu trn my xc nh nng ppmNO2 trong dung dch o, t suy ra hm lng NO2 trong mu
10TCN 452-2001 (C th dng thuc th Griss ci tin: Mc 6.2.2 thay bng thm vo mi bnh 1ml thuc th Sunfanylamit v 1ml thuc th N(1naphtyl) etylen diamine dihydrroclorua (NED)

6.3 Cng thc tnh ton: mg NO3-/ kg mu ti = a . V . 1000 v . m

Trong : a: hm lng NO3- trong th tch trch (mg) V: th tch dung dch mu sau khi chit (ml) v: th tch dung dch trch ra xc nh (ml) m: khi lng mu ti (g) K/T.b trng B Nng nghip v PTNT Th trng Ng Th Dn : k